Resíduos de agrotóxicos em ameixa, maçã, pera e pêssego: desenvolvimento de métodos de análise e monitoramento
Ano de defesa: | 2017 |
---|---|
Autor(a) principal: | |
Orientador(a): | |
Banca de defesa: | , , , |
Tipo de documento: | Tese |
Tipo de acesso: | Acesso aberto |
Idioma: | por |
Instituição de defesa: |
Universidade Federal de Santa Maria
Centro de Ciências Naturais e Exatas |
Programa de Pós-Graduação: |
Programa de Pós-Graduação em Química
|
Departamento: |
Química
|
País: |
Brasil
|
Palavras-chave em Português: | |
Palavras-chave em Inglês: | |
Área do conhecimento CNPq: | |
Link de acesso: | http://repositorio.ufsm.br/handle/1/12732 |
Resumo: | In recent years, the indiscriminate use of pesticides and a lack of adoption of good agricultural practices have been evidenced by the results of analyzes of residues of pesticides in food. Thus, the goal of this work was to develop and validate two methods for determination of pesticide residues in plum, apple, pear and peach, with analysis by ultra high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). In the development of the QuEChERS method, different conditions of the extract clean-up were tested. In the validation results, the linear range of the method was 5 to 200 μg kg-1 with recoveries were between 70 and 120% and RSD ≤20%. The practical limit of quantification (LOQ) for 161 compounds was 10 μg kg-1. In MSPD optimization, different sorbents (C18, florisil®, PSA, alumina, amino, silica, chitosan, Oasis® HLB, StrataTM-X and fluoridated) were tested as solid support in different proportions with the sample. The homogenization was carried out with metallic spheres and extraction with acetonitrile and ultrasound. Accuracy and precision results obtained by MSPD were adequate for 131 pesticides residues studied, with recovery results ranging between 70 and 120%, with RSD ≤ 20%. The studied compounds presented practical LOQ of 10 μg kg-1. In the analysis of 100 samples of the studied fruits, different pesticides residues were found in concentrations ranging from <LOQ to 2.334,6 μg kg-1. |
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2018-03-16T13:37:19Z2018-03-16T13:37:19Z2017-02-06http://repositorio.ufsm.br/handle/1/12732In recent years, the indiscriminate use of pesticides and a lack of adoption of good agricultural practices have been evidenced by the results of analyzes of residues of pesticides in food. Thus, the goal of this work was to develop and validate two methods for determination of pesticide residues in plum, apple, pear and peach, with analysis by ultra high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). In the development of the QuEChERS method, different conditions of the extract clean-up were tested. In the validation results, the linear range of the method was 5 to 200 μg kg-1 with recoveries were between 70 and 120% and RSD ≤20%. The practical limit of quantification (LOQ) for 161 compounds was 10 μg kg-1. In MSPD optimization, different sorbents (C18, florisil®, PSA, alumina, amino, silica, chitosan, Oasis® HLB, StrataTM-X and fluoridated) were tested as solid support in different proportions with the sample. The homogenization was carried out with metallic spheres and extraction with acetonitrile and ultrasound. Accuracy and precision results obtained by MSPD were adequate for 131 pesticides residues studied, with recovery results ranging between 70 and 120%, with RSD ≤ 20%. The studied compounds presented practical LOQ of 10 μg kg-1. In the analysis of 100 samples of the studied fruits, different pesticides residues were found in concentrations ranging from <LOQ to 2.334,6 μg kg-1.Nos últimos anos, o uso indiscriminado de agrotóxicos e a não adoção das boas práticas agrícolas têm sido evidenciados pelos resultados de análises de resíduos de agrotóxicos em alimentos. Assim, este trabalho teve como objetivo desenvolver e validar dois métodos para determinação de resíduos de agrotóxicos em ameixa, maçã, pera e pêssego, com análise por cromatografia líquida de ultra eficiência acoplada à espectrometria de massas em série (UHPLC-MS/MS). No desenvolvimento do método QuEChERS, diferentes condições da limpeza do extrato foram testadas. Nos resultados de validação, o intervalo linear do método foi de 5 a 200 μg kg-1, com recuperações entre 70 e 120% e RSD ≤ 20%. O limite de quantificação prático (LOQ) para 161 compostos foi de 10 μg kg-1. No desenvolvimento da técnica MSPD foram testados diferentes sorventes (C18, florisil®, PSA, alumina, amino, sílica, quitosana, Oasis® HLB, StrataTM-X e fase fluorada) como suporte sólido em diferentes proporções com a amostra. A homogeneização foi realizada com auxílio de esferas metálicas e a extração com acetonitrila e ultrassom. Os resultados de exatidão e precisão obtidos por MSPD foram adequados para resíduos de 131 agrotóxicos, com resultados de recuperação entre 70 e 120%, with RSD ≤ 20%. Os compostos estudados apresentaram LOQ prático de 10 μg kg-1. Na análise de 100 amostras das frutas estudadas, foram quantificados resíduos de diferentes agrotóxicos em concentrações entre <LOQ e 2.334,6 μg kg-1.porUniversidade Federal de Santa MariaCentro de Ciências Naturais e ExatasPrograma de Pós-Graduação em QuímicaUFSMBrasilQuímicaAttribution-NonCommercial-NoDerivatives 4.0 Internationalhttp://creativecommons.org/licenses/by-nc-nd/4.0/info:eu-repo/semantics/openAccessQuEChERSMSPDPreparo de amostraUHPLC-MS/MSAgrotóxicosSample preparationPesticidesFruitsCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAResíduos de agrotóxicos em ameixa, maçã, pera e pêssego: desenvolvimento de métodos de análise e monitoramentoPesticides residues in plum, apple, pear and peach: development of analytical methods and monitoringinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisZanella, Renatohttp://lattes.cnpq.br/2541865299438479Primel, Ednei Gilbertohttp://lattes.cnpq.br/3259602390948297Caldas, Sergiane Souzahttp://lattes.cnpq.br/5511956204092296Silva, Gustavo Pinto dahttp://lattes.cnpq.br/5659811271344671Prestes, Osmar Damianhttp://lattes.cnpq.br/9632234955509028http://lattes.cnpq.br/1096743335037955Kemmerich, Magali1006000000006000aa2baab-94e8-4d3d-bbb2-85495ba77db5a0398b1b-0b9e-4a5c-8286-f40fa9b1bc2ebaeb8541-95af-4405-96c9-db07639f33f696e9b42f-84a6-44f6-8017-a16a2cdfeeb31d59453a-755d-47d8-9f2f-2b4ed72793470496cf79-48da-4fcf-a75e-441d41336dd9reponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMCC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv |
Resíduos de agrotóxicos em ameixa, maçã, pera e pêssego: desenvolvimento de métodos de análise e monitoramento |
dc.title.alternative.eng.fl_str_mv |
Pesticides residues in plum, apple, pear and peach: development of analytical methods and monitoring |
title |
Resíduos de agrotóxicos em ameixa, maçã, pera e pêssego: desenvolvimento de métodos de análise e monitoramento |
spellingShingle |
Resíduos de agrotóxicos em ameixa, maçã, pera e pêssego: desenvolvimento de métodos de análise e monitoramento Kemmerich, Magali QuEChERS MSPD Preparo de amostra UHPLC-MS/MS Agrotóxicos Sample preparation Pesticides Fruits CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Resíduos de agrotóxicos em ameixa, maçã, pera e pêssego: desenvolvimento de métodos de análise e monitoramento |
title_full |
Resíduos de agrotóxicos em ameixa, maçã, pera e pêssego: desenvolvimento de métodos de análise e monitoramento |
title_fullStr |
Resíduos de agrotóxicos em ameixa, maçã, pera e pêssego: desenvolvimento de métodos de análise e monitoramento |
title_full_unstemmed |
Resíduos de agrotóxicos em ameixa, maçã, pera e pêssego: desenvolvimento de métodos de análise e monitoramento |
title_sort |
Resíduos de agrotóxicos em ameixa, maçã, pera e pêssego: desenvolvimento de métodos de análise e monitoramento |
author |
Kemmerich, Magali |
author_facet |
Kemmerich, Magali |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Zanella, Renato |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/2541865299438479 |
dc.contributor.referee1.fl_str_mv |
Primel, Ednei Gilberto |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/3259602390948297 |
dc.contributor.referee2.fl_str_mv |
Caldas, Sergiane Souza |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/5511956204092296 |
dc.contributor.referee3.fl_str_mv |
Silva, Gustavo Pinto da |
dc.contributor.referee3Lattes.fl_str_mv |
http://lattes.cnpq.br/5659811271344671 |
dc.contributor.referee4.fl_str_mv |
Prestes, Osmar Damian |
dc.contributor.referee4Lattes.fl_str_mv |
http://lattes.cnpq.br/9632234955509028 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/1096743335037955 |
dc.contributor.author.fl_str_mv |
Kemmerich, Magali |
contributor_str_mv |
Zanella, Renato Primel, Ednei Gilberto Caldas, Sergiane Souza Silva, Gustavo Pinto da Prestes, Osmar Damian |
dc.subject.por.fl_str_mv |
QuEChERS MSPD Preparo de amostra UHPLC-MS/MS Agrotóxicos |
topic |
QuEChERS MSPD Preparo de amostra UHPLC-MS/MS Agrotóxicos Sample preparation Pesticides Fruits CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Sample preparation Pesticides Fruits |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
In recent years, the indiscriminate use of pesticides and a lack of adoption of good agricultural practices have been evidenced by the results of analyzes of residues of pesticides in food. Thus, the goal of this work was to develop and validate two methods for determination of pesticide residues in plum, apple, pear and peach, with analysis by ultra high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). In the development of the QuEChERS method, different conditions of the extract clean-up were tested. In the validation results, the linear range of the method was 5 to 200 μg kg-1 with recoveries were between 70 and 120% and RSD ≤20%. The practical limit of quantification (LOQ) for 161 compounds was 10 μg kg-1. In MSPD optimization, different sorbents (C18, florisil®, PSA, alumina, amino, silica, chitosan, Oasis® HLB, StrataTM-X and fluoridated) were tested as solid support in different proportions with the sample. The homogenization was carried out with metallic spheres and extraction with acetonitrile and ultrasound. Accuracy and precision results obtained by MSPD were adequate for 131 pesticides residues studied, with recovery results ranging between 70 and 120%, with RSD ≤ 20%. The studied compounds presented practical LOQ of 10 μg kg-1. In the analysis of 100 samples of the studied fruits, different pesticides residues were found in concentrations ranging from <LOQ to 2.334,6 μg kg-1. |
publishDate |
2017 |
dc.date.issued.fl_str_mv |
2017-02-06 |
dc.date.accessioned.fl_str_mv |
2018-03-16T13:37:19Z |
dc.date.available.fl_str_mv |
2018-03-16T13:37:19Z |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/doctoralThesis |
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doctoralThesis |
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publishedVersion |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/12732 |
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http://repositorio.ufsm.br/handle/1/12732 |
dc.language.iso.fl_str_mv |
por |
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por |
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100600000000 |
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600 |
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Attribution-NonCommercial-NoDerivatives 4.0 International http://creativecommons.org/licenses/by-nc-nd/4.0/ info:eu-repo/semantics/openAccess |
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Attribution-NonCommercial-NoDerivatives 4.0 International http://creativecommons.org/licenses/by-nc-nd/4.0/ |
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openAccess |
dc.publisher.none.fl_str_mv |
Universidade Federal de Santa Maria Centro de Ciências Naturais e Exatas |
dc.publisher.program.fl_str_mv |
Programa de Pós-Graduação em Química |
dc.publisher.initials.fl_str_mv |
UFSM |
dc.publisher.country.fl_str_mv |
Brasil |
dc.publisher.department.fl_str_mv |
Química |
publisher.none.fl_str_mv |
Universidade Federal de Santa Maria Centro de Ciências Naturais e Exatas |
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